Measurement of Heteronuclear Bond Distances in Polycrystalline Solids by Solid-State NMR Techniques

James E. Roberts, Gerard S. Harbison, Michael G. Munowitz, Judith Herzfeld, Robert G. Griffin

Research output: Contribution to journalArticle

125 Citations (Scopus)

Abstract

High resolution dipolar/chemical shift NMR experiments for solids are critically reviewed and used to measure15N-!H bond distances in a series of compounds, many of which have also been studied by neutron diffraction. The results demonstrate that when recorded carefully, with attention paid to the experimental procedures described, two-dimensional dipolar/chemical shift spectra can yield bond distances accurate to within 0.005 A and mutual orientations of dipolar and chemical shift tensors accurate to within 3°. A comparison of the NMR distances with similar data from neutron diffraction experiments shows the NMR distances to be uniformly ~0.035 A longer, a result that is consistent with some vibrational averaging of the15N-'H dipolar interaction. Collectively, the experimental data and procedures described here demonstrate for the first time that high resolution dipolar/chemical shift NMR experiments are a viable method for locating protons in polycrystalline or amorphous solids. Previously, such determinations have been possible only with single crystal neutron diffraction techniques.

Original languageEnglish (US)
Pages (from-to)4163-4169
Number of pages7
JournalJournal of the American Chemical Society
Volume109
Issue number14
DOIs
StatePublished - Jul 1 1987

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Neutron Diffraction
Chemical shift
Neutron diffraction
Nuclear magnetic resonance
Protons
Experiments
Tensors
Single crystals

ASJC Scopus subject areas

  • Catalysis
  • Chemistry(all)
  • Biochemistry
  • Colloid and Surface Chemistry

Cite this

Measurement of Heteronuclear Bond Distances in Polycrystalline Solids by Solid-State NMR Techniques. / Roberts, James E.; Harbison, Gerard S.; Munowitz, Michael G.; Herzfeld, Judith; Griffin, Robert G.

In: Journal of the American Chemical Society, Vol. 109, No. 14, 01.07.1987, p. 4163-4169.

Research output: Contribution to journalArticle

Roberts, James E. ; Harbison, Gerard S. ; Munowitz, Michael G. ; Herzfeld, Judith ; Griffin, Robert G. / Measurement of Heteronuclear Bond Distances in Polycrystalline Solids by Solid-State NMR Techniques. In: Journal of the American Chemical Society. 1987 ; Vol. 109, No. 14. pp. 4163-4169.
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